High melting point rosin and method for its production



Patented Mar. 16, 1937- PATENT OFFICE men MELTING Poim' nosm AND Mc'rnop ron I rrs PRODUCTION Paul Sclmorl', Wiesli,

Hercules Powder Company, W a corporation of Delaware Swltierland, asslg nor to 'No Drawing. Application May 20; 1930, Serial No. 454,200. Renewed July iii-Claims.

My invention relatesto a high melting point rosin.and method for its production.

The method in accordance with my invention involves the treatment of wood or gum rosin, with reagentsand under conditions to be hereinafter fully disclosed, whereby its melting point is raised and the treated rosin is rendered adapt-- I able for many uses for which ordinary rosin is undesirable due to its relatively low melting 10 point. v

The rosin produced in; accordance with the method embodying this invention will be found to have a melting point within about the range 85 C.-100 C. (drop method) as compared with a melting point within about the range 76 C.-

79 C. (drop method) for untreated rosin. Gen

erally the treated rosin, have a-lower acid number than before treatment and while its color may be somewhat increased, it will not be black m or tarlike, but will rather be reddish in color when viewed in small particles. The rosin product may, if desired, be partially distilled, at suitable temperature and pressure, for its separa tioninto a soft rosin distillate and a hard rosin 25 residue i. e. comprising mainly rosin and polymerized rosin respectively. The hard rosin residue will amountQo about'25-75% of the product, de-' pending upon the condition of treatment.

In accordance with my invention rosin, either 7 wood or gum rosin, is subjected to t'reatment with a metallic chloride, preferably, though ,not necessarily, anhydrous, such, for example, as stannic chloride, aluminum chloride, zinc chloride, and the like; while at the same time the resin is heated without, however, subjecting it to a temperature such that any large proportion of thefrosln will be decomposed the metallic chloride acts catalytically to promote polymerization of therosin; g

- In carrying the method embodying my invention into practice, the rosin to be treated is desirablymelted, the metallic chloride added to it with agitation and the mixture then heated for say a period within about the range 0.5-10 hours, at a temperature-within about the range 100 C.--

200 (3., with 1 continued agitation to insure 'ef-j ficient contact between the rosin and the metal lic chloride. If desired, the product which will have a melting point, on completion of the treatment indicated, higher than that of the rosin subjected to treatment, may be partially distilled for its separation into'relatively hard and rela tively soft portions. Where either type, from the standpoint of hardness, is desirable for any par- 55 ticular use, when the product is partially distemperature within about the range 250 C.- 300C. under a reduced pressure within about .tilled such may desirably be eflected at a bath the range. /4 /g inch of mercury in order to avoid decomposition of the product;

As a more specific illustration of the practical adaptation of the method embodying this invention, for example, 150 grams of ordinary wood rosin, melting point 76- C.-79 C. (drop method) is melted, say at a temperature of about 125 C. and about 0.6 'cc. of stannic chloride added with agitation. The rosin is then subjected to treatment with the stannic chloride for a period of about nine hours, the temperature being'grad ually raised to about 150 C. and the agitation being continued. On completion of the treat-.- ment the-gproduct will be found to have a melting point .of about 93 0. (drop method), a somewhat lower acid number than the rosin treated and a reddish color. The product may be used where a high melting point required, as for example, in varnishes, ester gums and synthetic resins, and'the like. If desired the rosin may be subjected to treatment in solution in any suitable solvent, which will be inert in the treatment, as for example, gasoline, xylene, etc.

If desired, the'product may be partially distilled, for example, up to a bath temperature of about 300 C. under a pressure of about inch 0t mercury and under such conditions the'product may be made to 'separateinto a relatively soft distillate and a residue harder than and having,

avoided and the rosin is rather converted into a more complex compound by means .of polymerization than broken down into simpler substance by decomposition.

of apparatus will be required in carrying out the method embodying my invention.

\ Further, it will be understood that I contemplate as within the scope of my invention the use of any metallic chlorideoperably equivalent for those herein specifically mentioned. Thus, by wayof illustration, chlorides derived from a as has been indicated, a higher melting point It will be appreciated that no particular form position of any large proportion of the rosin is Y able, may be used equivalently for a 'ing an amphoteric hydroxide and with heat at a temperature below that at which any large proportion of the rosin will be decomposed but suilicient to effect polymerization in the presence of the metallic chloride, and iractionating the product to separate rosin from polymerized rosin.

2. The method of raising the melting point of rosin which includes treating rosin with an anhydrous metallic chloride derived from a metal capable of forming an amphoterichydroxide and with heat at a temperature below that at which any large proportion of the rosin will be decomposed but suilicient to effect polymerization in the presence of the metallic chloride, and subjecting the product to partial distillation at.a bath tem-- perature within about the range 250 C.-300 C. to-separate rosine from polymerized rosin.

3. The method of raising the melting point. of rosin which includes treating rosin with stannic chloride and with heat at a temperature within about the range 100 c.-o c. and subjectingthe product to partial. distillation under reduced pressure. a

4. The method of raising the melting point of rosin which includes treating rosin with stannic chloride and with heat at a temperaturegwithin about the range 100 C.-200 C. and subjecting the product to partial distillation under a'gpressure of about /2" of mercury up to a bath temperature of about 300 C.

5. The method 0! raising the melting point of rosin which includes treating rosin-with zinc chloride and with heat at a. temperature within about the range 100 (ll-200 C. and subjecting the product to partial distillation under redu e pressure.

6. The method of raislngthe melting point of rosin which includes treating rosin with zinc chloride and with heat at a'temperature within about the range 100 C.-200 C. and subjecting the product to partial distillationundeia pressure ot about be" 01' mercury up to a bath temperature of about 300 C.

"I. The method of raising the melting point of rosin .which includes-treating rosin with aluminum chloride and with heat at a temperature within about the range 100: C.-200 C. and subiecting the product to partial distillation under reduced pressure.

. 8. The method of raising the melting point of rosin which includes treating rosin with aluminum ,chloride and with heat at a temperature within about the range C.-200 Gland sub- 0 jecting the product to partial distillation under a pressure of about /2" of mercury up to a bath temperature of about 300 C.

9. The method of raising the melting point of rosin which includes treating rosin with'aluminumchloride and with heat at a temperature below that at which any large proportion of the by a higher melting point rosinwillbedbutsuflicienttoeliec polymerization in the presence of aluminum chloride and Iractionating the product to separate rosin from polymerized rosin.

10. The method or raising the melting point of rosin which includes treating rosin with zinc chloride and with heat at a temperature below that at which any large proportion of the rosin will be decomposed but sullicient to eflect polymerization in the presence of zinc chloride and iractionating the product to separate rosin from polymerized rosin.

11. The method of raising the melting point of rosin which includes treating rosin with stannic chloride and with heat at a temperature below that at which any large proportion of the-rosin will be decomposed but sufllcient to eflect' polymerization in the presence of stannic chloride and fractionating the product to separate rosin from polymerized rosin.

12. The method of raising the melting rosin which includes treating rosin with a volatile, inorganic metallic chloride derived from a metal capable of forming an amphoteric'hydroxide and with heat at, a temperature belowthat at which any large proportion or the resin.

will be decomposed'but sufllcient to eiIect polymerization in the presence of the metallic chloride; and fractionating the product to separate rosin Irom polymerized rosin,

- 13. The method of raising-the melting point of.

rosin which includes treating rosin with a volatile, inorganic metallic chloride derived from. 'a metal capable of forming an amphoteric hydroxide and with heat at a temperaturewithln about the range 100 C.-200 C. and fractionating the product to separate rosin from poly- 14. The method of raising the melting point of rosin which includes treating rosin in solution in an inert solvent for the rosin with a volatile, inorganic metallic chloride capable of forming an amphoteric hydroxide and with heat at a, temperature below that at which any large proportion of the rosin will be decomposed but sufllcient to eflect polymerization in the presence of the metallic chloride'and fractionating the product to separate resin from polymerized rodn.

' 15. A partially polymerized rosin characterized by a higher melting point than the rosin from which it is formed, said partially polymerized rosin being the residue left after iractional distillation under reduced pressure to remove the low end of the product formed by the treatment or rosin to eilect polymerization thereof.

16. A partially lymerized rosin characterized than therosin from which it is formed and by the presence oi traces (of a metallic chloride, said partially polymerized point oil derived from a metal 

